反应详情

To a mixture of 1-(3-methyl-4-nitrobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole (1.4 g), ammonium acetate (30.5 g), acetone (60 ml) and water (30 ml), 20% aqueous solution of titanium trichloride (27.5 g) was added at room temperature and the mixture was stirred at room temperature for 12 hours. After finishing the reaction, the mixture was extracted with ethyl acetate, washed with saturated aqueous solution of sodium chloride and dried with anhydrous sodium sulfate. After distilling off the solvent, the obtained residue was purified by silica gel column chromatography to obtain 1-(3-methyl-4-aminobenzyl)-3,5-bis(trifluoromethyl)-1H-pyrazole (1.19 g).

1. additionwas added at room temperature
2. customthe reaction
3. extractionthe mixture was extracted with ethyl acetate
4. washwashed with saturated aqueous solution of sodium chloride
5. dry with materialdried with anhydrous sodium sulfate
6. distillationAfter distilling off the solvent
7. customthe obtained residue was purified by silica gel column chromatography